Abstract: Titania nanoparticles co-doped with Ce³⁺, Fe³⁺, Zn²⁺ were prepared by sol-gel self-combustion synthesis with TiCl₄ as the precusor. The products were characterized by X-Ray Diffraction (XRD). The effects of Fe/Ce, (Fe + Ce)/Ti, citric acid/Ti (in mole ratio), calcining temperature and time on phase composition were investigated by the orthogonal experimental method. The results showed that citric acid/Ti, calcining temperature and (Fe + Ce)/Ti affect dominantly on phase composition of the products.